CN100390125C - Process for preparation of liquid metal carboxylate - Google Patents
Process for preparation of liquid metal carboxylate Download PDFInfo
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- CN100390125C CN100390125C CNB2003101078378A CN200310107837A CN100390125C CN 100390125 C CN100390125 C CN 100390125C CN B2003101078378 A CNB2003101078378 A CN B2003101078378A CN 200310107837 A CN200310107837 A CN 200310107837A CN 100390125 C CN100390125 C CN 100390125C
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- metal carboxylate
- liquid metal
- carboxylic acid
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Abstract
The present invention relates to a method for preparing liquid metal carboxylate, which comprises the steps that carboxylic acid reacts with alkali via saponification so as to generate sodium or potassium carboxylate, and the generated sodium or potassium carboxylate reacts with inorganic metal salt via double decomposition so as to generate liquid metal carboxylate, or the carboxylic acid directly reacts with metal oxides or hydroxides so as to generate the liquid metal carboxylate. Modification macaloid with 5 to 10mm of granularity and 4 to 8mm of pore size and No. 200 solvent oil are added in the reaction substances, reaction temperature is 80 to 120 DEG C, reaction time is 20 to 70 min, and the addition amount of the modification macaloid is 0.1 to 1%(weight) of the total amount of the reaction substances. After the reaction, lower layer water is removed by separation, and the reaction substances are filtered with heat so as to obtain yellowish vitreous liquid metal carboxylate products. The present invention makes use of micro holes of the macaloid to absorb impurity granules of inorganic salt, reduces the impurity content of the products, increases the transparence of the products and stabilizes product quality.
Description
Technical field
The present invention relates to a kind of preparation method of liquid metal carboxylate salt.
Background technology
Liquid metal carboxylate salt (Metal carboxylate) is the very important fine chemical product of a class, is mainly used in paint, ink drier, unsaturated polyester promotor, rubber bound promotor, fields such as stabilizer for plastics.
In the prior art, " development researches of the refining and series product of naphthenic acid " (Five City University's journal 2001,12, P51～54), " application of naphthenic acid salt and production " (lubricating oil, 1994,6, P43～46), " naphthenate technical study and exploration " (Hubei chemical industry, 1996,2, P31～33) etc. disclosed method is double decomposition and direct method.Their aftertreatment is to take water repeatedly to wash and stratified method in system, and shortcoming is that reaction time consumption is long, and can't guarantee the oarse-grained particle of unreacted and byproduct of reaction in the system of removing.This particle is present in the system very harmful, the first, they can slowly gather, and become macroparticle, can influence after in the adding system goods gloss; The second, they are very easily water-soluble inorganic metal salts, add in the hydrophobic systems, and after the system for the treatment of was solidified, the dawn runs into water will be got off by water dissolution, makes system tiny cavity occur, influences products appearance and shortens its working life.
Summary of the invention
In order to overcome the defective in the prior art, the invention provides a kind of preparation method of new liquid metal carboxylate salt.This method is simple to operate, and is with short production cycle, with low cost, and good product quality is applicable to industrial production.
Method of the present invention realizes by adding a kind of modification infusorial earth in the reaction later stage, the preparation method of this liquid metal carboxylate salt, comprise that the alkali with carboxylic acid and sodium or potassium carries out saponification reaction, carboxylic acid sodium salt that generates or sylvite carry out replacement(metathesis)reaction with inorganic metal salt again and generate the liquid metal carboxylate, or with carboxylic acid and metal oxide or oxyhydroxide direct reaction generation liquid metal carboxylate.Be characterized in: constantly stir and stop, add modification infusorial earth and No. 200 solvent oils in above-mentioned reactant, temperature of reaction is 80～120 ℃, and the reaction times is 20～70 minutes, and the add-on that changes bio-diatomite is 0.1～1% weight percent of reactant gross weight; After reaction is finished, separate sub-cloud water, filtered while hot gets light yellow transparent liquid carboxylate metal product salt.
The granularity of the modification infusorial earth among the present invention is 5～10 microns, and the aperture is 4～8 microns, and rate of permeation is 15～20 darcies (Darcy).
Carboxylic acid among the present invention is naphthenic acid or isocaprylic acid.Naphthenic acid is the byproduct in the petroleum refining, and it is a kind of mixture of carboxylic acids with five-ring or six-ring, and the molecule of isocaprylic acid is CH
3CH
2CH
2CH
2CH (C
2H
5) COOH.
Alkali among the present invention is solid or liquid sodium hydroxide or potassium hydroxide.
Inorganic metal salt among the present invention is to choose any one kind of them in the vitriol of cobalt, manganese, lead, zinc, calcium or hydrochloride and the zirconium oxychloride.
Metal oxide among the present invention or oxyhydroxide are to choose any one kind of them in plumbous oxide, zinc oxide, calcium hydroxide, hydrated barta, the Vanadium Pentoxide in FLAKES.
The preparation method of liquid metal carboxylate salt of the present invention adopts and adds organic phase and the inorganic phase interface area that modification infusorial earth increases reaction, utilize diatomaceous micropore to adsorb the inorganic salt impurity particle, remove by filter diatomite then, the solution colour after the filtration is more shallow, and outward appearance is more transparent.
The present invention compared with prior art has following advantage: one, transparency of products improves, and foreign matter content reduces, constant product quality.Two, owing to having reduced water-washing step, simple to operate.Three, with short production cycle, shortened to 7 hours from original 24 hours.Four, it is nearly 70% to have reduced discharge of wastewater, has protected ecotope.
Embodiment
Below by embodiment content of the present invention is further described, but embodiment is not a limitation of the present invention.
Embodiment 1
In having churned mechanically there-necked flask, add the 40g tap water, isocaprylic acid 290g, solid sodium hydroxide 80g opens and stirs, and is warming up to 90 ℃, add No. 200 solvent oil 100g after 10 minutes, add the 110g Calcium Chloride Powder Anhydrous again, 100 ℃ are incubated one hour, add modification infusorial earth 0.5g, take out sub-cloud water after, filtered while hot, get light yellow transparent liquid 500g, calcium contents 7.5%, yield 93.8%, 7 microns of maximum contaminant fineness.
Embodiment 2
In having churned mechanically there-necked flask, add the 40g tap water, isocaprylic acid 290g, solid sodium hydroxide 80g opens and stirs, and is warming up to 90 ℃, add No. 200 solvent oil 100g after 10 minutes, add the 110g Calcium Chloride Powder Anhydrous again, 100 ℃ are incubated one hour, add modification infusorial earth 2.5g, take out sub-cloud water after, filtered while hot, get light yellow transparent liquid 502g, calcium contents 7.82%, yield 98.1%, 5 microns of maximum contaminant fineness.
Embodiment 3
In having churned mechanically there-necked flask, add the 40g tap water, isocaprylic acid 290g, solid sodium hydroxide 80g opens and stirs, and is warming up to 90 ℃, add No. 200 solvent oil 100g after 10 minutes, add the 110g Calcium Chloride Powder Anhydrous again, 100 ℃ are incubated one hour, add modification infusorial earth 5g, take out sub-cloud water after, filtered while hot, get light yellow transparent liquid 500g, calcium contents 7.89%, yield 98.6%, 4 microns of impurity fineness.
Embodiment 4
In having churned mechanically there-necked flask, add isocaprylic acid 290g, solid hydrogen calcium oxide 74g, No. 200 solvent oil 100g, open and stir, be warming up to 100 ℃ of insulations one hour, add modification infusorial earth 2.5g, after taking out sub-cloud water, filtered while hot gets light yellow transparent liquid 500g, calcium contents 7.89%, yield 98.6%, 5 microns of impurity fineness.
Embodiment 5
In having churned mechanically there-necked flask, add naphthenic acid 582g (acid number 193mgKOH/g), solid hydrogen calcium oxide 74g, No. 200 solvent oil 100g, open and stir, be warming up to 100 ℃ of insulations one hour, add modification infusorial earth 2.5g, after taking out sub-cloud water, filtered while hot gets light yellow transparent liquid 780g, calcium contents 5.03%, yield 98%, 5 microns of impurity fineness.
Claims (4)
1. the preparation method of a liquid metal carboxylate salt, comprise that the alkali with carboxylic acid and sodium or potassium carries out saponification reaction, carboxylic acid sodium salt that generates or sylvite carry out replacement(metathesis)reaction with inorganic metal salt again and generate the liquid metal carboxylate, or generate the liquid metal carboxylate with carboxylic acid and metal oxide or oxyhydroxide direct reaction, it is characterized in that: stir down, in above-mentioned reactant, add modification algae soil and No. 200 solvent oils, temperature of reaction is 80～120 ℃, reaction times is 20～70 minutes, and the add-on of modification infusorial earth is 0.1～1% weight percent of reactant gross weight; After reaction is finished, separate sub-cloud water, filtered while hot gets faint yellow transparent liquid metal carboxylate salt product; Described carboxylic acid is naphthenic acid or isocaprylic acid, and described inorganic metal salt is to choose any one kind of them in the vitriol of cobalt, manganese, lead, zinc, calcium or hydrochloride and the zirconium oxychloride.
2. the preparation method of metal carboxylate according to claim 1, it is characterized in that: the granularity of described modification infusorial earth is 5～10 microns, and the aperture is 4～8 microns, and rate of permeation is 15～20 darcies.
3. the preparation method of metal carboxylate according to claim 1 and 2, it is characterized in that: described alkali is solid or liquid sodium hydroxide or potassium hydroxide.
4. the preparation method of metal carboxylate according to claim 1 and 2, it is characterized in that: described metal oxide or oxyhydroxide are: choose any one kind of them in plumbous oxide, zinc oxide, calcium hydroxide, hydrated barta, the Vanadium Pentoxide in FLAKES.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101078378A CN100390125C (en) | 2003-10-10 | 2003-10-10 | Process for preparation of liquid metal carboxylate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101078378A CN100390125C (en) | 2003-10-10 | 2003-10-10 | Process for preparation of liquid metal carboxylate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1605582A CN1605582A (en) | 2005-04-13 |
| CN100390125C true CN100390125C (en) | 2008-05-28 |
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|---|---|---|---|
| CNB2003101078378A Expired - Fee Related CN100390125C (en) | 2003-10-10 | 2003-10-10 | Process for preparation of liquid metal carboxylate |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106542987B (en) * | 2016-09-29 | 2019-04-19 | 沈阳化工大学 | A method of preparing cobalt laurate |
| CN111718655A (en) * | 2020-07-01 | 2020-09-29 | 中山华明泰科技股份有限公司 | Preparation method and application of composite calcium iso-octoate |
| CN114702637A (en) * | 2022-04-01 | 2022-07-05 | 国科广化韶关新材料研究院 | Preparation method and application of environment-friendly polyurethane catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5145488A (en) * | 1989-09-28 | 1992-09-08 | Hoechst Aktiengesellschaft | Process for the preparation of mixtures of oil-soluble iron and magnesium salts of saturated aliphatic monocarboxylic acids and their use |
| CN1218452A (en) * | 1996-03-29 | 1999-06-02 | 罗狄亚公司 | Synthesis of solid, powdery rare earth carboxylates by precipitation method |
-
2003
- 2003-10-10 CN CNB2003101078378A patent/CN100390125C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5145488A (en) * | 1989-09-28 | 1992-09-08 | Hoechst Aktiengesellschaft | Process for the preparation of mixtures of oil-soluble iron and magnesium salts of saturated aliphatic monocarboxylic acids and their use |
| CN1218452A (en) * | 1996-03-29 | 1999-06-02 | 罗狄亚公司 | Synthesis of solid, powdery rare earth carboxylates by precipitation method |
Non-Patent Citations (2)
| Title |
|---|
| 异辛酸钴合成工艺的研究. 贺晓慧.石油化工，第28卷第3期. 1999 |
| 异辛酸钴合成工艺的研究. 贺晓慧.石油化工，第28卷第3期. 1999 * |
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Owner name: SHANGHAI HUAYI FINE CHEMICAL INDUSTRY CO., LTD. Free format text: FORMER NAME: SHANGHAI PAINT CO., LTD. |
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Address after: 201108 Shanghai city Minhang District humin Road Town Patentee after: SHANGHAI HUAYI FINE CHEMICAL CO., LTD. Address before: 200020 Shaanxi South Road, Shanghai, No. 345 Patentee before: Shanghai Paint Co., Ltd. |
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